CN108793228A - A kind of synthetic method of carbon-coated indium oxide hollow bar - Google Patents
A kind of synthetic method of carbon-coated indium oxide hollow bar Download PDFInfo
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- CN108793228A CN108793228A CN201810705939.6A CN201810705939A CN108793228A CN 108793228 A CN108793228 A CN 108793228A CN 201810705939 A CN201810705939 A CN 201810705939A CN 108793228 A CN108793228 A CN 108793228A
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- indium oxide
- carbon
- indium
- oxide hollow
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention discloses a kind of synthetic method of carbon-coated indium oxide hollow bar, includes the following steps：The first step：It takes four nitric hydrate indiums and terephthalic acid (TPA) to be dissolved in n,N-Dimethylformamide solution, stirs evenly, above-mentioned mixed solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, is heated to required temperature and required reaction time.Product is collected by centrifugation, is then washed product for several times with industrial alcohol, you can obtain the MOF of the uniform indium of scale topography, second step：The obtained uniform hexagonal nano stick of scale topography, chooses suitable calcination temperature, calcination time and calcination atmosphere are calcined in tube furnace, you can obtain carbon-coated indium oxide hollow nanorod.Carbon coating of the present invention can improve the separative efficiency of electrons and holes, while increase the stability of oxidation indium nanometer particle, prevent its reunion, hollow-core construction from can increase specific surface area, increase the active site of reaction.
Description
Technical field
The present invention relates to a kind of synthetic methods of carbon-coated indium oxide hollow bar.
Background technology
Metal-organic framework (MOFs) material is that one kind for being self-assembly of by inorganic metal ion and organic ligand is new
The hybrid inorganic-organic materials of type.Compared with traditional inorganic porous material, it have higher specific surface area, porosity and
The duct of rule, and its structure and properties is easy to regulate and control.Metal oxide nano-material is in air-sensitive, photocatalysis, photodissociation aquatic products hydrogen
Etc. be widely used.Indium oxide semiconductor makees photochemical catalyst, and there are many problems, and the utilization ratio such as incident light is low, photoproduction
The low separation efficiency of electrons and holes, material prepared specific surface area is smaller, and the active site of reaction is less etc., for existing
These problems, general solution is carried noble metal at present, particle size is done it is small etc., but a disadvantage is that noble metal cost compared with
Height, particle is smaller easily to reunite, and catalytic effect decreases.In view of the above problems, we invent it is a kind of carbon-coated
Indium oxide hollow nanorod, carbon coating can improve the separative efficiency of electrons and holes, while increase oxidation indium nanometer particle
Stability prevents its reunion, hollow-core construction from can increase specific surface area, increases the active site of reaction.Synthesize at present this
The method of carbon-coated indium oxide hollow nanorod has not been reported.
Invention content
The object of the present invention is to provide a kind of simple synthesis size is smaller, pattern is uniform, and carbon-coated indium oxide is hollow
The method of nanometer rods.
Include the following steps：
The first step：Appropriate four nitric hydrates indium and terephthalic acid (TPA) is taken to be dissolved in N,N-dimethylformamide solution, stirring is equal
It is even, above-mentioned mixed solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, when being heated to required temperature and required reaction
Between.Product is collected by centrifugation, is then washed product for several times with industrial alcohol, you can obtain the uniform indium of scale topography
MOF；
Second step：The obtained uniform hexagonal nano stick of scale topography chooses suitable calcination temperature, calcination time and calcining gas
Atmosphere is calcined in tube furnace, you can obtains carbon-coated indium oxide hollow nanorod.
Carbon coating of the present invention can improve the separative efficiency of electrons and holes, while increase the stabilization of oxidation indium nanometer particle
Property, it prevents its reunion, hollow-core construction from can increase specific surface area, increases the active site of reaction.Pass through the simple hydro-thermal of a step
The indium base MOF nanometer rods to size uniformity of reaction.Using indium base MOF nanometer rods as template, by calcining obtain carbon coating and in
The indium oxide micron bar of hollow structure.
Description of the drawings
The X-ray powder diffraction figure (XRD) of Fig. 1 (a) predecessor indium bases MOF；(b) scanning electron microscope of predecessor indium base MOF
Scheme (SEM).
The X-ray powder diffraction figure of indium oxide nanometer rods after Fig. 2 (a) calcinings（Black）And indium oxide standard X-ray powder
Diffraction pattern（It is red）(XRD)；(b) scanning electron microscope (SEM) photograph (SEM) of rodlike indium oxide after calcining.
Fig. 3 low power transmission electron microscope pictures.
The scanning electron microscope (SEM) photograph (SEM) of reaction temperature products different Fig. 4.
The Product scan electron microscope (SEM) that reaction time different Fig. 5 obtains.
The scanning electron microscope (SEM) photograph (SEM) of Fig. 6 difference calcination temperature products.
The scanning electron microscope (SEM) photograph (SEM) of Fig. 7 difference calcination time products.
Specific implementation mode
A kind of synthetic method of carbon-coated indium oxide hollow bar,
Include the following steps：
Take four nitric hydrate indiums（0.018mmol）And terephthalic acid (TPA)（0.02mmol）It is dissolved in 10mlN, dinethylformamide
It in solution, stirs evenly, above-mentioned mixed solution is transferred in 50ml reaction kettles, be heated to 100-120 DEG C, reaction time 4-
6h.Product is collected by centrifugation, is then washed product for several times with industrial alcohol；
The In- base MOF predecessors after appropriate drying are taken to be placed in tube furnace, with vacuum pump by tube furnace vacuum state, with 5
DEG C/heating of the speed of min, temperature reaches 500-550 DEG C, maintains 1-2h, room temperature is down to the speed of 5 DEG C/min.
The synthesis predecessor experiment reaction temperature of the present invention can be obtained of uniform size rodlike within the scope of 100-120 DEG C
In bases MOF.
The X-ray powder diffraction figure (XRD) of Fig. 1 (a) predecessor indium bases MOF；(b) scanning electron microscope of predecessor indium base MOF
Scheme (SEM).
Fig. 1 is the XRD (Fig. 1 a) and scanning electron microscope (SEM) photograph of the product of gained under the conditions of the above-mentioned experiment first step（Fig. 1 b）.
XRD diagram shows that products therefrom is MOF-68, and scanning electron microscope (SEM) photograph shows that products therefrom is six rib micron bars of size uniform.
The X-ray powder diffraction figure of indium oxide nanometer rods after Fig. 2 (a) calcinings（Black）And indium oxide standard X-ray powder
Diffraction pattern（It is red）(XRD)；(b) scanning electron microscope (SEM) photograph (SEM) of rodlike indium oxide after calcining.
Fig. 2 is the XRD (Fig. 2 a) and scanning electron microscope (SEM) photograph of the product of gained under the conditions of above-mentioned experiment second step（Fig. 2 b）.
XRD diagram shows that products therefrom is indium oxide, and scanning electron microscope (SEM) photograph shows that club shaped structure can substantially be kept after calcining, rodlike surface
Become coarse by smooth.
Fig. 3 is In2O3/ C low power transmission electron microscope pictures,
Indium oxide nanometer rods after figure calcining carry out the characterization of low power transmission electron microscope, it was demonstrated that obtain during Rod-like shape keeps substantially
The micron bar of hollow structure.The characterization of high power transmission is carried out to the part of indium oxide nanometer rods, it was demonstrated that after calcining, nanorod surfaces
It is to be accumulated by little particle.The size of the granule on its surface is counted, the little particle that size is more than 10 nanometers.Figure pair
The surface of rodlike indium oxide carries out high-resolution, it was demonstrated that is coated with one layer of thin carbon outside little particle, electronic diffraction further proves small
Particle is the nano particle of indium oxide.
The scanning electron microscope (SEM) photograph (SEM) of reaction temperature products different Fig. 4.
Reaction temperature is the scanning electron microscope (SEM) photograph of 100 DEG C of products（Fig. 4 a）；Reaction temperature is the scanning electron microscope (SEM) photograph of 110 DEG C of products
（Fig. 4 b）；Reaction temperature is the scanning electron microscope (SEM) photograph of 120 DEG C of products（Fig. 3）.The product obtained by the above differential responses temperature is swept
Electron microscope is retouched, shows that rodlike In bases of uniform size can be obtained in the experiment reaction temperature of the present invention within the scope of 100-120 DEG C
MOFs。
2. rodlike In bases of uniform size can be obtained in the synthesis predecessor experiment reaction time in the present invention within the scope of 4-6h
MOF。
The Product scan electron microscope (SEM) that reaction time different Fig. 5 obtains.
Reaction time is the scanning electron microscope (SEM) photograph of 4h products（Fig. 5 a）；Reaction temperature is the scanning electron microscope (SEM) photograph of 5h products（Figure
5b）；Reaction time is the scanning electron microscope (SEM) photograph of 6h products（Fig. 5 c）.The Product scan Electronic Speculum obtained by the above differential responses time
Figure shows that rodlike In bases MOF of uniform size can be obtained in the experiment reaction time of the present invention within the scope of 4-6h.
3. carbon packet of uniform size can be obtained in present invention calcining predecessor experiment reaction temperature within the scope of 500-550 DEG C
Cover the indium oxide micron bar of hollow structure.The scanning electron microscope (SEM) photograph (SEM) of Fig. 6 difference calcination temperature products.
Calcination temperature is the scanning electron microscope (SEM) photograph of 500 DEG C of products（Fig. 6 a）；Reaction temperature is the scanning electron microscope (SEM) photograph of 550 DEG C of products
（Fig. 6 b）.The Product scan electron microscope obtained by the above different calcination temperatures, shows that the experiment calcination temperature of the present invention exists
The indium oxide nanometer rods of carbon coating hollow structure of uniform size can be obtained within the scope of 500-550 DEG C.
It is hollow that carbon coating of uniform size can be obtained in the calcining predecessor experiment reaction time in the present invention within the scope of 1-6h
The indium oxide micron bar of structure.
The scanning electron microscope (SEM) photograph (SEM) of Fig. 7 difference calcination time products.
When calcination temperature is 550 DEG C, calcination time is the scanning electron microscope (SEM) photograph of 1h products（Fig. 7 a）；Calcination temperature is 550 DEG C
When, calcination time is the scanning electron microscope (SEM) photograph of 3h products（Fig. 7 b）；When calcination temperature is 550 DEG C, calcination time is sweeping for 6h products
Retouch electron microscope（Fig. 7 c）；Pass through the Product scan under above 550 DEG C of the calcination temperature, obtained by the different calcination times of 1-6h
Electron microscope shows that carbon coating hollow structure of uniform size can be obtained in the experiment calcination temperature of the present invention within the scope of 1-6h
Indium oxide micron bar.
Compared with prior art：MOF nanometers of the indium base to size uniformity that the present invention passes through the simple hydro-thermal reaction of a step
Stick.
Using indium base MOF nanometer rods as template, the indium oxide micron bar of carbon coating and hollow structure is obtained by calcining.
Claims (3)
1. a kind of synthetic method of carbon-coated indium oxide hollow bar, which is characterized in that include the following steps：
The first step：It takes appropriate four nitric hydrates indium and terephthalic acid (TPA) to be dissolved in N,N-dimethylformamide solution to stir
It is even, above-mentioned mixed solution is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, when being heated to required temperature and required reaction
Between, product is collected by centrifugation, is then washed product for several times with industrial alcohol, you can obtain the uniform indium of scale topography
MOF；
Second step：The obtained uniform hexagonal nano stick of scale topography chooses suitable calcination temperature, calcination time and calcining gas
Atmosphere is calcined in tube furnace, you can obtains carbon-coated indium oxide hollow nanorod.
2. a kind of synthetic method of carbon-coated indium oxide hollow bar according to claim 1, it is characterised in that：Described
Four nitric hydrate indium 0.018mmol, terephthalic acid (TPA) 0.02mmol.
3. a kind of synthetic method of carbon-coated indium oxide hollow bar according to claim 1, it is characterised in that：Second step
Middle calcination temperature is 500-550 DEG C, maintains 1-2h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205686A (en) * | 2018-11-21 | 2019-01-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nickel oxide based on MOF/indium sesquioxide heterojunction nanometer material preparation method and product and application |
| CN109821526A (en) * | 2019-02-20 | 2019-05-31 | 北京工业大学 | A kind of preparation method for constructing metal-doped indium oxide photocatalyst based on heteronuclear MOFs template |
| CN109999780A (en) * | 2019-05-05 | 2019-07-12 | 江苏师范大学 | In with double-shell structure2O3The synthetic method of micro-and nanorods |
| CN110615464A (en) * | 2019-10-23 | 2019-12-27 | 江苏师范大学 | In wrapped by nitrogen and sulfur element doped carbon layer2O3Hollow nanosphere and preparation method thereof |
| CN117691096A (en) * | 2024-02-04 | 2024-03-12 | 内蒙古工业大学 | Silicon-based composite anode material of all-solid-state lithium battery and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668612A (en) * | 2016-03-15 | 2016-06-15 | 济南大学 | Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor |
| CN106057490A (en) * | 2016-07-21 | 2016-10-26 | 中国石油大学(华东) | Nano oxide based on metal-organic frameworks (MOFs) and preparation method thereof |
| CN106450227A (en) * | 2016-11-24 | 2017-02-22 | 福建师范大学 | Method for preparing lithium batteries by hierarchy In2O3/C composite materials |
| CN107032389A (en) * | 2017-06-16 | 2017-08-11 | 宁波大学 | A kind of porous oxidation indium nano material and preparation method thereof |
-
2018
- 2018-06-26 CN CN201810705939.6A patent/CN108793228A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668612A (en) * | 2016-03-15 | 2016-06-15 | 济南大学 | Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor |
| CN106057490A (en) * | 2016-07-21 | 2016-10-26 | 中国石油大学(华东) | Nano oxide based on metal-organic frameworks (MOFs) and preparation method thereof |
| CN106450227A (en) * | 2016-11-24 | 2017-02-22 | 福建师范大学 | Method for preparing lithium batteries by hierarchy In2O3/C composite materials |
| CN107032389A (en) * | 2017-06-16 | 2017-08-11 | 宁波大学 | A kind of porous oxidation indium nano material and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205686A (en) * | 2018-11-21 | 2019-01-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nickel oxide based on MOF/indium sesquioxide heterojunction nanometer material preparation method and product and application |
| CN109821526A (en) * | 2019-02-20 | 2019-05-31 | 北京工业大学 | A kind of preparation method for constructing metal-doped indium oxide photocatalyst based on heteronuclear MOFs template |
| CN109999780A (en) * | 2019-05-05 | 2019-07-12 | 江苏师范大学 | In with double-shell structure2O3The synthetic method of micro-and nanorods |
| CN109999780B (en) * | 2019-05-05 | 2021-02-12 | 江苏师范大学 | In having a double-layer shell structure2O3Synthesis method of micro-nano rod |
| CN110615464A (en) * | 2019-10-23 | 2019-12-27 | 江苏师范大学 | In wrapped by nitrogen and sulfur element doped carbon layer2O3Hollow nanosphere and preparation method thereof |
| CN117691096A (en) * | 2024-02-04 | 2024-03-12 | 内蒙古工业大学 | Silicon-based composite anode material of all-solid-state lithium battery and preparation method thereof |
| CN117691096B (en) * | 2024-02-04 | 2024-04-09 | 内蒙古工业大学 | Silicon-based composite anode material of all-solid-state lithium battery and preparation method thereof |
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